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Method for preparing special aromatic polyoxadiazole and flame-retardant high-temperature resistant polyoxadiazole fiber thereof

A polyoxadiazole and aromatic technology, applied in the direction of fiber chemical characteristics, wet spinning method, single-component synthetic polymer rayon, etc., can solve the problem of unstable performance, difficult control of one or two substitutions, polymer structure Complicated issues

Active Publication Date: 2012-07-11
JIANGSU BAODE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former uses flame-retardant modified terephthalic acid as a flame-retardant monomer, the synthesis process is complicated, and the primary or secondary substitution is difficult to control, resulting in complicated polymer structure and unstable performance, and more than 10% bromine content is required to achieve flame retardancy. Combustion effect (LOI ≥ 30%), the fiber produces a large amount of hydrogen bromide poisonous gas during the combustion process

Method used

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  • Method for preparing special aromatic polyoxadiazole and flame-retardant high-temperature resistant polyoxadiazole fiber thereof
  • Method for preparing special aromatic polyoxadiazole and flame-retardant high-temperature resistant polyoxadiazole fiber thereof
  • Method for preparing special aromatic polyoxadiazole and flame-retardant high-temperature resistant polyoxadiazole fiber thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Example 1. Using oleum as a solvent to prepare halogen-containing flame-retardant and high-temperature-resistant polyoxadiazole fibers and their special POD polymers

[0066] Polyoxadiazole fibers can be figure 1 The process flow diagram shown in the preparation.

[0067] 1. Preparation of POD polymer

[0068] Preparation of Flame Retardant Modified Monomer

[0069] Pass bromine into a closed reaction kettle containing isophthalic acid and oleum, and use FeCl 3 or FeBr 3 As a catalyst, it was stirred and reacted at 120°C for 5 hours, and excess gas was removed after the reaction to obtain Br-containing flame-retardant modified isophthalic acid. The equivalent ratio (molar ratio) of each reactant is: isophthalic acid: SO 3 :Br 2 : FeCl 3 (FeBr 3 )=1:20:1.2:0.05. Tested with an ultraviolet spectrophotometer, the halogen substitution rate is 85-95%.

[0070] Polymerization of POD solution

[0071] Hydrazine sulfate (NH 2 NH 2 .H 2 SO 4 ) dissolved in SO at 8...

Embodiment 2

[0082] Example 2, using fuming sulfuric acid as a solvent to prepare phosphorus-containing flame-retardant and high-temperature-resistant polyoxadiazole fibers and their special POD polymers

[0083] 1. Preparation of POD polymer

[0084] Preparation of Flame Retardant Modified Monomer

[0085] Dissolve diphenyloxy(sulfur)phosphine in dioxane (Dioxane), and then add catalyst AlCl to the solvent 3 , and m-xylene was slowly added dropwise under reflux at 85°C. After the dropwise addition, reflux reaction was carried out for 6 hours. After the reaction was completed, a pure m-xylene substitute was obtained by washing and recrystallization. The m-xylene substitute is oxidized twice with potassium permanganate to obtain a flame-retardant isophthalic acid monomer substituted by diphenyl (sulfur) phosphine, and the molar ratio of each reactant is: solvent: AlCl 3 : Substituent: m-xylene=15:1.15:1.5:1, the molar ratio of the amount of potassium permanganate twice to the monomer (m-x...

example 3

[0088] Example 3, polyphosphoric acid is used as a solvent to prepare halogen-containing flame-retardant and high-temperature-resistant polyoxadiazole fibers and their special POD polymers

[0089] 1. Preparation of POD polymer

[0090] The preparation of the flame retardant modified monomer is the same as in Example 1.

[0091] Polymerization of POD solution

[0092] Hydrazine sulfate (NH 2 NH 2 .H 2 SO 4 ) dissolved in P at 110°C 2 o 5 In polyphosphoric acid with a mass percent content of 80% and a degree of polymerization of 4, terephthalic acid and Br-containing flame-retardant modified isophthalic acid (the compound in which R is Br in formula I) are sequentially added, and various reactions The molar ratio is P 2 o 5 : terephthalic acid: flame retardant modified isophthalic acid: hydrazine sulfate = 10: 0.90: 0.10: 1.02. The reaction temperature in the pre-polymerization stage is 110°C, and the reaction time is 4h; the reaction temperature in the polymerization...

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Abstract

The invention discloses a method for preparing special aromatic polyoxadiazole and flame-retardant high-temperature resistant polyoxadiazole fiber thereof. The special aromatic polyoxadiazole is prepared by the following method that the special aromatic polyoxadiazole is prepared from terephthalic acid, compound of which the structural general formula is expressed as formula I and hydrazine salt serving as monomers through condensation polymerization reaction. The polyoxadiazole fiber with high flame retardancy and high temperature resistance is prepared by using the special aromatic polyoxadiazole as a raw material. The fiber number of the prepared polyoxadiazole fiber is 1 to 20 dtex, the breaking strength is 2.5 to 5 cN.dtex-1, the elongation at break is 10 to 40 percent, the initial modulus is 50 to 250 cN.dtex-1, the moisture regain is 5.0 to 12.0 percent, the limited oxygen index is 30 to 38 percent, and the initial decomposition temperature is above 480 DEG C. The fiber can be widely used in the fields of protective products, filter materials, electric insulating materials, frictional sealed materials, various industrial textiles, high-temperature resistant paper, aviation and aerospace materials and the like.

Description

technical field [0001] The invention relates to a special aromatic polyoxadiazole and a method for preparing the flame-retardant and high-temperature-resistant polyoxadiazole fiber. Background technique [0002] Aromatic polyoxadiazole (POD for short) is an aromatic heterocyclic polymer material with good heat resistance, oxidation resistance, chemical corrosion resistance and electrical insulation properties. It is insoluble in general organic solvents and most inorganic solvents. It only decomposes but does not melt at high temperature, so it has broad application prospects in high temperature resistance, electrical insulation and other fields. However, due to its difficulty in synthesis, poor fluidity, and difficulty in processing and molding, there are relatively few research and development achievements in the synthesis of POD polymers and fiber molding. [0003] The preparation and research of aromatic polyoxadiazoles began in the 1960s and was first initiated by the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/08D01F6/74D01D5/06
Inventor 徐建军周国泰施楣梧张再兴叶光斗姜猛进吴萌李守群
Owner JIANGSU BAODE NEW MATERIAL
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